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Oxygen-resistant molybdenum phosphide catalyst

A molybdenum phosphide catalyst, catalyst technology, applied in the direction of carbon compound catalyst, catalyst, physical/chemical process catalyst, etc., can solve the problem of difficult passivation layer thickness, and achieve the effect of excellent oxygen resistance

Inactive Publication Date: 2017-11-17
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, this is only a method to protect the phosphide catalyst in a short period of time. Not only is the thickness of the passivation layer difficult to control, but it cannot fundamentally overcome the shortcoming of the bulk phase being oxidized during long-term storage.

Method used

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  • Oxygen-resistant molybdenum phosphide catalyst
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  • Oxygen-resistant molybdenum phosphide catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] MoP was prepared by temperature-programmed reduction of phosphate precursors.

[0034] At room temperature, 2.57 grams of ammonium heptamolybdate ((NH 4 ) 6 Mo 7 o 24 4H 2 O) and 3.56 grams of diammonium phosphate ((NH 4 ) 2 HPO 4 ) was added to 20mL deionized aqueous solution, dissolved to obtain a clear and transparent solution, the solution was placed in an oven at 120°C for 12 hours to dry the moisture, and the obtained solid was roasted at 500°C for 6 hours to obtain the oxide precursor of MoP, wherein Mo The / P molar ratio was 1.

[0035] The phosphide catalyst was prepared by in-situ temperature-programmed reduction method. The temperature programming step mainly includes two steps: (1) in H 2 Under the atmosphere (flow rate 150mL / min), the temperature was raised from room temperature to 120°C at 5°C / min, and kept at 120°C for 1 hour to remove the water adsorbed by the catalyst; (2) from 120°C to 5°C / min. to 400°C, then the temperature was raised from 4...

Embodiment 2

[0037] MoP prepared by temperature-programmed reduction of sulfur-containing precursors.

[0038] 3.8 grams of ammonium heptamolybdate ((NH 4 ) 6 Mo 7 o 24 4H 2 O) be dissolved in 10ml ammonia water for subsequent use. 22 grams of ammonium sulfide ((NH 4 ) 2 S) Dissolve in 50mL of deionized water, then place in an ice bath, and slowly add 6.6mL of phosphorus trichloride (PCl 3 ) solution (95.5% in water). After the dropwise addition was completed, the ice bath was removed, and the ammonia solution of ammonium molybdate obtained before was slowly added dropwise to it. After reacting at room temperature for 1 hour, the three-necked flask was placed in the refrigerator until the crystals were completely formed. Suction filtration, the upper filter cake is washed with ethanol / water and then dried to obtain the catalyst precursor.

[0039] The phosphide catalyst was prepared by in-situ temperature-programmed reduction method. The temperature programming step mainly includ...

Embodiment 3

[0044] Ni 2 P 2 S 6 Reduction to prepare sulfur-containing Ni 2 P catalyst.

[0045] 75 grams of sodium sulfide (Na 2 S·9H 2 O) Dissolve in 100mL deionized water, then place in an ice bath, and slowly add 6.6mL of phosphorus trichloride (PCl 3 ) solution (95.5% in water). After the dropwise addition was completed, the ice bath was removed, and after reacting at room temperature for 1 hour, the three-neck flask was placed in the refrigerator until white crystals were completely formed. Then suction filtration, after the obtained white substance is recrystallized with ethanol / hot water solution, Na 4 P 2 S 6 The hydrate of Na can be obtained after drying 4 P 2 S 6 white solid. 1.8 g of Na 4 P 2 S 6 With 1.88 grams of nickel chloride (NiCl 2 ·6H 2 O) After fully grinding, put it into the quartz tube of the tube furnace, continuously feed high-purity nitrogen, treat it at 500 ° C for 10 hours, wash with ethanol / water solution and dry to obtain Ni 2 P 2 S 6 bla...

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Abstract

The invention relates to an oxygen-resistant molybdenum phosphide catalyst, which contains sulfur, wherein the sulfur is distributed on the surface and the bulk phase of molybdenum phosphide. According to the present invention, the disclosed molybdenum phosphide catalyst has excellent oxygen resistance, the catalytic activity of the oxygen-resistant molybdenum phosphide catalyst is not substantially affected after the oxygen-resistant molybdenum phosphide catalyst is stored in the air for a long time, and the oxygen-resistant molybdenum phosphide catalyst does not require the pre-reduction activation when the oxygen-resistant molybdenum phosphide catalyst is used in hydrogenation, hydrodesulfurization, hydrodenitrogenation and other hydrogen present reactions.

Description

technical field [0001] The invention belongs to the technical field of heterogeneous catalysis, and in particular relates to a molybdenum phosphide solid catalyst for hydrogenation reaction. Background technique [0002] Metal-rich transition metal phosphides (Ni 2 P, MoP and WP, ​​etc.) have the characteristics of metals, and are used in hydrogenation (Catal. .2000,191:438), hydrodeoxygenation (J.Catal.2014,318:151.), hydrazine decomposition (J.Catal.2007,249:397) and hydrogen evolution (Angew.Chem.Int.Ed.2014, 53:14433; Appl.Catal.B:Env,2016,196:193) and other important reactions catalyzed by metal catalysts under hydrogen-free and oxygen-free conditions have good application prospects. Among these phosphide catalysts, MoP exhibits excellent performance in hydrodenitrogenation, hydrazine decomposition, and hydrogen evolution reactions. The main problem restricting the application of transition metal phosphides is that the preparation conditions of these catalysts are ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/19C07C5/11C07C13/48
CPCB01J27/19C07C5/11C07C2527/19C07C13/48
Inventor 李翔田松王安杰
Owner DALIAN UNIV OF TECH
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